Salting-out-assisted liquid-liquid extraction as a suitable approach for determination of methoxetamine in large sets of tissue samples
The result's identifiers
Result code in IS VaVaI
<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F60461373%3A22340%2F16%3A43901617" target="_blank" >RIV/60461373:22340/16:43901617 - isvavai.cz</a>
Alternative codes found
RIV/60461373:22330/16:43901617 RIV/00023752:_____/16:43914931
Result on the web
<a href="http://dx.doi.org/10.1007/s00216-015-9221-1" target="_blank" >http://dx.doi.org/10.1007/s00216-015-9221-1</a>
DOI - Digital Object Identifier
<a href="http://dx.doi.org/10.1007/s00216-015-9221-1" target="_blank" >10.1007/s00216-015-9221-1</a>
Alternative languages
Result language
angličtina
Original language name
Salting-out-assisted liquid-liquid extraction as a suitable approach for determination of methoxetamine in large sets of tissue samples
Original language description
A new designer drug, a dissociative anesthetic, and a putative N-methyl-d-aspartate receptor antagonist, methoxetamine (MXE) noted by the EU Early Warning System has been already identified as a cause of several fatalities worldwide. The primary objective of this work was to develop a suitable sample preparation method allowing for isolation of MXE and its main metabolites in high yields from rat brain, liver, and lungs. For the purpose of the project, MXE and five metabolites were synthesized in-house, specifically O-desmethyl-normethoxetamine, O-desmethylmethoxetamine, dihydro-O-desmethylmethoxetamine, normethoxetamine, and dihydromethoxetamine. A sample preparation procedure consisted in the homogenization of the tissue applying salting-out-assisted liquid-liquid extraction (SALLE). A subsequent liquid chromatography-mass spectrometry (LC-MS) analysis was based on reversed-phased chromatography hyphenated with a triple quad MS system in a positive electrospray mode. Multiple reaction monitoring (MRM) was used for qualification and quantification of the analytes. The quantification was based on the application of an isotopically labeled internal standard, normethoxetamine-d(3). The matrix-matched calibrations were prepared for each type of matrix with regression coefficients 0.9943-1.0000. The calibration curves were linear in the concentration range of 2.5-250 ng g(-1). Limits of quantification (LOQs) were estimated as 2.5 and 5 ng g(-1), respectively. Recovery (80-117 %) and matrix effect (94-110 %) at 100 ng g(-1) and intra- and inter-day accuracy and precision at low (2.5 ng g(-1)), middle (25 ng g(-1)), and upper (250 ng g(-1)) concentration levels for all the analytes in all three types of tissues were also determined. The developed analytical method was applied to a set of real samples gathered in toxicological trials on rats and MXE, and its metabolites were determined successfully.
Czech name
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Czech description
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Classification
Type
J<sub>x</sub> - Unclassified - Peer-reviewed scientific article (Jimp, Jsc and Jost)
CEP classification
CE - Biochemistry
OECD FORD branch
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Result continuities
Project
<a href="/en/project/VG20122015075" target="_blank" >VG20122015075: New synthetic drugs (NSD) - creation of toxicological database, development and validation of detection methods including fast imunochemical tests, behavioral pharmacology, pharmacokinetics and biotransformation in rats, epidemiology</a><br>
Continuities
S - Specificky vyzkum na vysokych skolach
Others
Publication year
2016
Confidentiality
S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů
Data specific for result type
Name of the periodical
Analytical and Bioanalytical Chemistry
ISSN
1618-2642
e-ISSN
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Volume of the periodical
408
Issue of the periodical within the volume
4
Country of publishing house
DE - GERMANY
Number of pages
10
Pages from-to
1171-1181
UT code for WoS article
000368720600014
EID of the result in the Scopus database
2-s2.0-84958104896